Ammonium Acetate → HCID 86667580, 화합물

HRID 85287노트

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HRID 85287 반응식
[CH2:1]([N:5]([CH2:25][CH2:26][CH2:27][CH3:28])[C:6]1[CH:11]=[CH:10][C:9]([CH:12]=[CH:13][CH:14]=[CH:15][C:16]2[S:20][C:19]([CH:21]=O)=[CH:18][CH:17]=2)=[C:8]([O:23][CH3:24])[CH:7]=1)[CH2:2][CH2:3][CH3:4].[C:29]([C:31]1[C:32](=[C:39]([C:42]#[N:43])[C:40]#[N:41])[O:33][C:34]([CH3:38])([CH3:37])[C:35]=1[CH3:36])#[N:30].C([O-])(=O)C.[NH4+]>C(O)C.O1CCCC1>[CH2:25]([N:5]([CH2:1][CH2:2][CH2:3][CH3:4])[C:6]1[CH:11]=[CH:10][C:9]([CH:12]=[CH:13][CH:14]=[CH:15][C:16]2[S:20][C:19]([CH:21]=[CH:36][C:35]3[C:34]([CH3:37])([CH3:38])[O:33][C:32](=[C:39]([C:40]#[N:41])[C:42]#[N:43])[C:31]=3[C:29]#[N:30])=[CH:18][CH:17]=2)=[C:8]([O:23][CH3:24])[CH:7]=1)[CH2:26][CH2:27][CH3:28]

참가 물질

6

반응물 3

HCID 517165Ammonium AcetateHCID 99903452-[3-Cyano-4,5,5-trimethylfuran-2(5H)-ylidene]malononitrileHCID 86667579HCID 86667579, 화합물

생성물 1

HCID 86667580HCID 86667580, 화합물수율 68.3%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

In 7 ml of ethanol and 2 ml of tetrahydrofuran were dissolved 248 mg (0.62 mmol) of 5-[4-(4-dibutylamino-2-methoxyphenyl)-1,3-butadienyl]thiophene-2-carboaldehyde and 137 mg (0.61 mmol) of 2-(3-cyano-4,5,5-trimethyl-2(5H)-furanylidene) propanedinitrile. To this mixture was added 50 mg of ammonium acetate, and the mixture was stirred with heating at 50° C. for 4 hours. The product was separated by filtration, washed with ethanol, and purified by silica gel column chromatography to give 241 mg of a dark brown crystal (yield: 66.8%; mp: 185-187° C.)

후처리

  1. customThe product was separated by filtration
  2. washwashed with ethanol
  3. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-ccda706d73a74925b683dd618937ada3
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846955B2

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